CN111235521B - Preparation method of SIH film and preparation method of infrared band-pass multilayer film - Google Patents
Preparation method of SIH film and preparation method of infrared band-pass multilayer film Download PDFInfo
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- CN111235521B CN111235521B CN202010045219.9A CN202010045219A CN111235521B CN 111235521 B CN111235521 B CN 111235521B CN 202010045219 A CN202010045219 A CN 202010045219A CN 111235521 B CN111235521 B CN 111235521B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3485—Sputtering using pulsed power to the target
Abstract
A preparation method of an SIH film and a preparation method of an infrared band-pass multilayer film belong to the technical field of film coating. The preparation method of the SIH membrane comprises the following steps: step S01, vacuumizing a cavity of the sputtering film plating machine; step S02, placing the glass substrate in a film coating chamber for heating; step S03, carrying out ICP ion pre-cleaning on the glass substrate by using plasma gas Ar; step S04, Ar and H2 are filled in the vicinity of the target material, and Ar and H2 are used for bombarding the Si target in the direct current pulse mode to form an SIH film on the bottom of the glass substrate. The preparation method of the infrared band-pass multilayer film comprises the following steps: step S10, preparing a SIH film on a glass substrate by the above method; step S20, filling Ar and O2 into the cavity, and bombarding the Si target with Ar to generate a SiO2 film; and step S30, repeating the steps S10-S20 to form the infrared band-pass multilayer film. The invention has low production cost and high productivity, and can produce SIH film with N >3.68 and k <0.0002 and infrared band-pass filter with low angle effect.
Description
Technical Field
The invention belongs to the technical field of coating, and particularly relates to a preparation method of an SIH film and a preparation method of an infrared band-pass multilayer film.
Background
The prior art has two methods for preparing SIH materials by using a relaxation sputtering coating machine. Firstly, Si atoms are deposited on a glass substrate by sputtering a high-purity spray Si target by using a laser sputtering machine, Ar and other gases of H2 and O2 in different proportions are filled in a coating chamber, an SIH material containing oxygen is generated under the action of plasma, and the SIH material has the characteristics of refractive index n being greater than 3.35, extinction coefficient k being less than 0.0001 and the like. Secondly, a specially modified sputtering machine is used for sputtering a high-purity binding Si target, Ar and H2 are filled in the vicinity of the target, SIH molecules are deposited on a glass substrate through the oxidation-reduction reaction of plasma gas, and the prepared SIH material has the characteristics that n is greater than 3.68, and k is less than 0.0002. The material prepared by the first method has a low refractive index, a large-angle offset of 11.5-12nm is formed when the infrared band-pass filter is prepared, the refractive index is low, the film layer is thick, and the manufacturing cost is high. The material prepared by the second method has a large refractive index, but the adopted sputtering machine is foreign imported equipment, the equipment cost is more than 2000 ten thousand yuan, and the equipment productivity is low.
The invention patent application CN201910414368.5 discloses a method for manufacturing an infrared narrow-band filter, and specifically discloses a method comprising the following steps: and coating a film by a medium-frequency sputtering mode, and directly filling hydrogen into the target in the sputtering process of the target to react to obtain the high-refractive-index SIH material layer with aluminum, wherein the target is a silicon-aluminum target. The intermediate frequency sputtering mode comprises the following steps: the film is sputtered from top to bottom, wherein a sputtering source is arranged on the upper part, and a substrate is arranged on the lower part. The refractive index of the SIH material prepared by the method is only above 3.5, and is lower than that of the material prepared by the second method.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of an SIH film and a preparation method of an infrared band-pass multilayer film, which have low cost and high productivity, so as to obtain the SIH film with high refractive index and the infrared band-pass filter with low angle effect.
The invention is realized by the following technical scheme:
the invention relates to a preparation method of an SIH membrane, which comprises the following steps:
step S01, vacuumizing a cavity of the sputtering film plating machine;
step S02, placing the glass substrate in a film coating chamber for heating;
step S03, carrying out ICP ion pre-cleaning on the glass substrate by using plasma gas Ar;
step S04, Ar and H2 are filled in the vicinity of the target material, and Ar and H2 are used for bombarding the Si target in the direct current pulse mode to form an SIH film on the bottom of the glass substrate.
The method has simple process and low cost.
Preferably, in the step S01, the cavity is vacuumized to 4E-4 to 2.0E-3 Pa.
Preferably, the step S02 includes: the glass substrate is placed in a film coating chamber for heating at the temperature of 150 ℃ and 250 ℃ for 30 min-2H.
Preferably, the step S03 includes: and (2) utilizing Plasma gas Ar, controlling the flow rate to be 100-.
Preferably, the step S04 includes: filling Ar of 20-200sccm and H2 of 5-100sccm into the vicinity of the target material, bombarding the Si target by using Ar and H2 in a direct current pulse mode, reacting to generate an SIH material, and depositing the SIH material on the bottom of the glass substrate to form the SIH film.
Preferably, the refractive index n of the formed SIH film is greater than 3.68, and the extinction coefficient k is less than 0.0002.
A method of making an infrared bandpass multilayer film, comprising:
step S10 of preparing a SIH film on a glass substrate by the method of claim 1;
step S20, filling Ar and O2 into the cavity, and bombarding the Si target with Ar to generate a SiO2 film;
and step S30, repeating the steps S10-S20 to form the infrared band-pass multilayer film.
Preferably, the sequence of step S10 and step S20 may be reversed.
Preferably, the step S20 includes: ar of 100sccm-800sccm and O2 of 100sccm-400sccm are filled in the cavity, Ar gas is used for bombarding the Si target, Si molecules are deposited on the bottom of the glass substrate, and then the SiO2 film is generated through the action of the Si target and O2.
Preferably, the method is used for preparing a near-infrared or mid-infrared or infrared long-wave pass filter or a narrow-band filter.
The invention has the following beneficial effects:
according to the preparation method of the SIH film and the preparation method of the infrared band-pass multilayer film, the heater and TG direct current pulse sputtering are simply added on the existing photothyreoscope, and hydrogen is charged nearby the target material, so that the SIH film with the characteristics that N is greater than 3.68 and k is less than 0.0002 can be prepared; and an infrared band pass filter having a lower angle effect was prepared using the SIH film and the SIO2 film. The preparation method is simple, the cost is 5-6 times lower than that of the existing product, the industrial manufacturing cost is reduced, and the productivity is high.
Drawings
FIG. 1 is a flow chart of a method for preparing an SIH membrane according to the present invention;
FIG. 2 is a schematic structural diagram of a conventional sputtering coater;
FIG. 3 is a schematic structural diagram of a photorelaxation sputtering coating machine for preparing an SIH film and an infrared band-pass multilayer film by adopting the method of the invention;
FIG. 4 is a graph showing the transmittance and reflectance profiles of a single-layer SIH film prepared by a method for preparing an SIH film according to the present invention;
FIG. 5 is a graph of a multilayer film made using an infrared bandpass multilayer film fabrication method of the present invention.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
Referring to fig. 1, a method for preparing a SIH film of the present invention includes:
step S01, vacuumizing a cavity of the sputtering film plating machine;
step S02, placing the glass substrate in a film coating chamber for heating;
step S03, carrying out ICP ion pre-cleaning on the glass substrate by using plasma gas Ar;
step S04, Ar and H2 are filled in the vicinity of the target material, and Ar and H2 are used for bombarding the Si target in the direct current pulse mode to form an SIH film on the bottom of the glass substrate.
The step S01 includes: and vacuumizing the cavity to 4E-4-2.0E-3 Pa.
The step S02 includes: the glass substrate is placed in a film coating chamber for heating at the temperature of 150 ℃ and 250 ℃ for 30 min-2H.
The step S03 includes: and utilizing plasma gas Ar to control the flow rate to be 100 and 800sccm, and carrying out ICP ion precleaning on the glass substrate for 1-10 min.
The step S04 includes: ar of 20-200sccm and H of 5-100sccm are charged in the vicinity of the target material2In DC pulse mode with Ar and H2The Si target is bombarded out and reacted to produce the SIH material, which is deposited onto the substrate of the glass substrate to form a SIH film. Form aThe refractive index n of the SIH film is greater than 3.68 and the extinction coefficient k is less than 0.0002.
In addition, other functional films, such as high reflection films HR, black films, multi-band-pass narrow-band films and the like, can be designed by utilizing the preparation method of the SIH film.
The invention also provides a preparation method of the infrared band-pass multilayer film, which comprises the following steps:
step S10, preparing the SIH film on the glass substrate by adopting the method;
step S20, filling Ar and O2 into the cavity, and bombarding the Si target with Ar to generate a SiO2 film;
and step S30, repeating the steps S10-S20 to form the infrared band-pass multilayer film.
In step S10, the SIH single layer film has the characteristics of N >3.68, K <0.0002 at 940nm, and the single layer film is prepared with a wavelength shift of less than 11nm at incident light angle variations of 0 to 30.
The step S20 includes: ar of 100sccm-800sccm and O2 of 100sccm-400sccm are filled in the cavity, Ar gas is used for bombarding the Si target, Si molecules are deposited on the bottom of the glass substrate, and then the SiO2 film is generated through the action of the Si target and O2. The multilayer film product produced by the method comprises optical filters of near infrared and mid-infrared narrow bands, infrared long wave pass, narrow bands and the like. The cut-off depths of two sides (visible light and infrared light) of the pass band of the optical filter prepared by the method are high in OD5-OD6 level, the blue shift of the wavelength of 0-30 degrees of low large-angle shift is less than 11nm, (the blue shift of the wavelength of 0-60 degrees is less than 27nm, the angle shift is not limited to 30 degrees), the gradient of the curve is high, the gradient of T10-T90 is less than 8nm, the highest point of the transmittance of the curve can reach 98%, and the average transmittance of the pass band is greater than 95%. In this way, stray light and wide angle effects of the product can be reduced.
The method can be realized based on the existing relaxed sputtering film plating machine. A heater and a TG direct current pulse sputtering mode are added on the basis of the prior film coating machine shown in figure 2. Specifically, (1) a coating chamber: the vacuum is between 2.0E-03Pa and 1.0E-05 Pa; (2) target material: high purity Si target, purity>99.99%, there are various sputtering modes, alternating current and direct current pulse modes; (3) ICP: inductively coupling the plasma, introducing H2Reacting with Si molecule to generate SiH film, introducing O2Can react with Si molecule to generateTo SiO2A film; (4) substrate: the clean substrate needing film coating can be a glass substrate made of different materials, a high-temperature resistant plastic substrate, a sapphire substrate and other materials; (5) a heater: heating means for heating the chamber. Based on the improvement of the equipment, hydrogen is charged near each target material, and Ar and H are utilized in a direct current pulse mode2Bombarding the target material to generate the SIH film.
The refractive index of the single layer SIH calculated by the optical layer optical design software from the transmission and reflection curves of the single layer film shown in fig. 4 is shown in the following table: at 942.9nm, the SIH has N3.695 and k 0.000171.
Table-table of refractive index n and extinction coefficient of single layer film calculated based on optilayer optical design software
The curve of the multilayer film designed and prepared from the single layer film is shown in fig. 5:
the spectrum of the multilayer film has the following characteristics:
380nm-750nm Tave<0.0001％
750nm-905nm Tmax<0.01％，Tave<0.001％
934nm-962nm Tave〉95％(AOI＝0°),925nm-951nm Tave>95％(AOI＝30°)
Slop T10-T90<8nm
1000nm-1100nm Tmax<0.01％，Tave<0.001％。
0°-30°Shift(T90)<11nm
it will be appreciated by persons skilled in the art that the embodiments of the invention described above and shown in the drawings are given by way of example only and are not limiting of the invention. The objects of the present invention have been fully and effectively accomplished. The functional and structural principles of the present invention have been shown and described in the examples, and any variations or modifications of the embodiments of the present invention may be made without departing from the principles.
Claims (5)
1. A method for preparing an SIH film, comprising:
step S01, vacuumizing a cavity of the sputtering film plating machine; in the step S01, the cavity is vacuumized to 4E-4-2.0E-3 Pa;
step S02, placing the glass substrate in a film coating chamber for heating; the step S02 includes: placing the glass substrate in a coating chamber for heating at the temperature of 150 ℃ and 250 ℃ for 30min-2 h;
step S03, carrying out ICP ion pre-cleaning on the glass substrate by using plasma gas Ar; the step S03 includes: plasma precleaning the glass substrate for 1-10min by using plasma gas Ar with the flow rate of 100-800sccm and the ICP power of 0.5-4 kW;
step S04, Ar and H are charged near the target material2In DC pulse mode with Ar and H2Bombarding the Si target to form an SIH film on the substrate of the glass substrate; the step S04 includes: ar of 20-300sccm and H of 5-100sccm are charged in the vicinity of the target2In DC pulse mode with Ar and H2The Si target is bombarded and reacted to produce the SIH material, which is deposited onto a substrate of a glass substrate to form a SIH film.
2. The method of claim 1, wherein the refractive index n of the SIH film is greater than 3.68 and the extinction coefficient k is less than 0.0002.
3. A method for preparing an infrared band-pass multilayer film is characterized by comprising the following steps:
step S10 of preparing a SIH film on a glass substrate by the method of claim 1;
step S20, filling Ar and O into the cavity2To form SiO2A film; the step S20 includes: ar of 100sccm-800sccm and 100sccm-400sccmO are charged into the chamber2Bombarding Si target with Ar gas to deposit Si molecule on the substrate of glass substrate, and passing through the Si target and O2Act to form SiO2A film;
and step S30, repeating the steps S10-S20 to form the infrared band-pass multilayer film.
4. The method of claim 3, wherein the sequence of steps S10 and S20 is reversed.
5. The method for preparing an infrared band-pass multilayer film according to claim 3, wherein the method is used for preparing a near-infrared or mid-infrared long-wave pass filter or a narrow-band filter.
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| CN107841712A (en) * | 2017-11-01 | 2018-03-27 | 浙江水晶光电科技股份有限公司 | Preparation method, high index of refraction hydrogenated silicon film by utilizing, optical filtering lamination and the optical filter of high index of refraction hydrogenated silicon film by utilizing |
| CN110579829A (en) * | 2018-07-26 | 2019-12-17 | 蓝思科技（长沙）有限公司 | Near-infrared filter, preparation method thereof and filtering equipment |
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| CN107841712A (en) * | 2017-11-01 | 2018-03-27 | 浙江水晶光电科技股份有限公司 | Preparation method, high index of refraction hydrogenated silicon film by utilizing, optical filtering lamination and the optical filter of high index of refraction hydrogenated silicon film by utilizing |
| CN110579829A (en) * | 2018-07-26 | 2019-12-17 | 蓝思科技（长沙）有限公司 | Near-infrared filter, preparation method thereof and filtering equipment |
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